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Preparation method of gabapentin intermediate

A technology for gabapentin and intermediates, which is applied in the field of preparation of gabapentin intermediates, can solve the problems of cumbersome steps, unfavorable industrial production, and expensive raw materials, and achieve the effects of shortened steps, low cost, and mild conditions

Active Publication Date: 2021-04-02
内蒙古永太化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The yield of this invention is greater than 96%, the content of 1,1-cyclohexyl diacetic acid monoamide in the product is greater than 99.7%, and the product quality is good; but the raw materials used in this application are relatively expensive, which is not conducive to industrial production
[0005] There are also some preparation methods that need to synthesize the intermediate cyclohexyl diacetic acid first, and then react to synthesize cyclohexyl diacetic acid monoamide, and the steps are more loaded down with trivial details

Method used

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  • Preparation method of gabapentin intermediate
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  • Preparation method of gabapentin intermediate

Examples

Experimental program
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Effect test

Embodiment 1

[0076] Embodiment 1 A kind of preparation method of gabapentin intermediate

[0077] Specifically include the following steps:

[0078] (1) Cool down to below 10°C, add 249g of 70% cyanoacetic acid aqueous solution to the lye prepared by water (210g) and sodium hydroxide (90g) and mix to form cyanoacetic acid alkali solution; control the internal temperature to 15°C , slowly drop cyclohexanone (98g) into the cyanoacetic acid alkali solution, after the dropwise addition, keep stirring for 8h to obtain reactant A;

[0079] (2) After the heat preservation is over, control the internal temperature not to be higher than 35°C, slowly add concentrated sulfuric acid (300g) dropwise to the reactant A, raise the temperature to about 30°C and stir for half an hour, then stir at 40°C for 4 hours to obtain the reactant B ;

[0080] (3) Cool down to 20-30°C, add toluene (300g) to the reactant B and extract twice, separate the organic phase and the aqueous phase, concentrate the organic ph...

Embodiment 2

[0086] Embodiment 2 A kind of preparation method of gabapentin intermediate

[0087] Specifically include the following steps:

[0088] (1) Cool down to below 10°C, mix 249g of 70% cyanoacetic acid aqueous solution with the lye prepared by adding water (210g) and sodium carbonate (140g), and configure it into cyanoacetic acid alkali solution; control the internal temperature to 30°C, and Cyclohexanone (98g) was slowly added dropwise into the cyanoacetic acid alkali solution, and after the dropwise addition was completed, it was incubated and stirred for 8 hours to obtain reactant A;

[0089] (2) After the heat preservation is over, control the internal temperature not to be higher than 35°C, slowly add 36% concentrated hydrochloric acid (300g) dropwise to the reactant A, heat up to 40°C and stir for half an hour, then stir at 60°C for 4 hours to obtain the reaction Object B;

[0090] (3) cooling to 20-30° C., adding ethyl acetate (300 g) to the reactant B and extracting twic...

Embodiment 3

[0094] Embodiment 3 A kind of preparation method of gabapentin intermediate

[0095] Specifically include the following steps:

[0096] (1) Cool down to below 10°C, mix 249g of 70% cyanoacetic acid aqueous solution with the lye prepared by adding water (210g) and sodium bicarbonate (189g), and configure it into cyanoacetic acid alkaline solution; control the internal temperature to 15°C, Slowly add cyclohexanone (98g) dropwise to the cyanoacetic acid alkali solution, after the dropwise addition, keep stirring for 8h to obtain reactant A;

[0097] (2) After the heat preservation is over, control the internal temperature not higher than 35°C, slowly add 85% concentrated phosphoric acid (346g) dropwise to the reactant A, heat up at 30°C and stir for half an hour, then stir at 40°C for 4 hours to obtain the reaction Object B;

[0098] (3) cooling to 20-30 DEG C, adding xylene (300g) to the reactant B and extracting twice, separating the organic phase and the aqueous phase, conce...

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Abstract

The invention provides a preparation method of a gabapentin intermediate, and relates to the field of chemical organic synthesis. The preparation method comprises the following steps: taking cyanoacetic acid and cyclohexanone as raw materials, carrying out condensation, hydrolysis and decarboxylation reactions to obtain imide in an intermediate body, and further carrying out alkaline hydrolysis toobtain the intermediate cyclohexyl diacetate monoamide. The preparation method of the gabapentin intermediate provided by the invention has the advantages of readily available raw materials, mild reaction conditions, high safety factor, strong operability, simple process, easiness in industrialization, high product purity and stable quality.

Description

technical field [0001] The invention relates to the field of chemical organic synthesis, more specifically, the invention relates to a preparation method of a gabapentin intermediate. Background technique [0002] Gabapentin (Gabapentin) is an antiepileptic drug first developed by Warner-Lanbert in the United States. It was first listed in the UK in 1993. Gabapentin is a novel antiepileptic drug. It is a white to off-white crystalline powder with a molecular formula of C 9 h 17 NO 2 , with a molecular weight of 171.23700, a melting point of 162°C, and a boiling point of 314.4°C (760mmHg). It is used for epilepsy patients with localized seizures that cannot be satisfactorily controlled or tolerated by conventional antiepileptic drugs, and localized seizures followed by generalized epilepsy. Additional treatment. Gabapentin is a structural analogue of an important neurotransmitter γ-aminobutyric acid (GABA) in mammals. It mainly exerts pharmacological effects by changing th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/14C07C233/08
CPCC07D221/20C07C231/14C07C253/30C07C2601/14C07C233/08C07C255/19C07C255/31
Inventor 卫禾耕孔佳辉张冲夏海建王学进
Owner 内蒙古永太化学有限公司
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